CN113000340B - Optically variable coating and preparation method thereof - Google Patents
Optically variable coating and preparation method thereof Download PDFInfo
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- CN113000340B CN113000340B CN202110224660.8A CN202110224660A CN113000340B CN 113000340 B CN113000340 B CN 113000340B CN 202110224660 A CN202110224660 A CN 202110224660A CN 113000340 B CN113000340 B CN 113000340B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/186—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof from or via fluosilicic acid or salts thereof by a wet process
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2203/00—Other substrates
- B05D2203/30—Other inorganic substrates, e.g. ceramics, silicon
- B05D2203/35—Glass
Abstract
The invention discloses an optically variable coating and a preparation method thereof, the method has the advantages of easily available raw materials, simple process, low cost, low energy consumption and easy realization, and the silicon dioxide particles with normal distribution characteristics of particle size are generated by taking tetraethoxysilane as a silicon source, absolute ethyl alcohol as a solvent and ammonia water as a catalyst. Preparing a silica colloid solution with a certain mass fraction, and self-assembling the silica colloid solution on a transparent film substrate to generate the structural color of the silica photonic crystal. The whole preparation method is mild in reaction condition and easy to implement, adopts a precursor multi-step dropping method, controls the synthesis rate of the silicon dioxide by bidirectional dropping in the reaction process, and finally prepares the angle-dependent silicon dioxide photonic crystal, so that the structural color can be cyclically changed in the whole visible light range, and the effect of observing the dynamic conversion of the iridescence by naked eyes is realized.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the technical field of photonic crystals, and particularly relates to an optically variable coating and a preparation method thereof.
[ background of the invention ]
The photonic crystal is an optical material formed by orderly and alternately arranging micro-nano materials with different refractive indexes in a three-dimensional space, can shield light with specific frequency from propagating in the structure, and the light with the specific frequency interacts with the photonic crystal structure to generate refraction, diffuse reflection and coherent diffraction, so that a bright structural color visible to naked eyes is formed finally. At present, the photonic crystal with the color change effect is mainly stimulated by two ways of physics and chemistry. The physical stimulation is mainly based on physical color generated by interaction of light and a microstructure of the photonic crystal material, and the structural color changes along with the angle of incident light, but the problem that the color changes narrowly in the visible wavelength range exists at present.
[ summary of the invention ]
The invention aims to overcome the defects of the prior art and provides an optically variable coating and a preparation method thereof, so as to solve the problem that the structural color in the visible wavelength range is narrow in change in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a method for preparing an optically variable coating comprises the following steps:
step 1, mixing absolute ethyl alcohol, deionized water and ammonia water, adding tetraethoxysilane, and reacting to generate a reaction solution A;
step 2, mixing absolute ethyl alcohol, deionized water and ammonia water, and then dropwise adding the reaction solution A to form a reaction solution B;
step 3, adding absolute ethyl alcohol and ammonia water into water to form a reaction solution C; dropwise adding ethyl orthosilicate and the reaction solution C into the reaction solution B, and reacting to generate a solution D;
step 4, washing the solution D with ethanol, centrifuging, and drying the centrifuged product to obtain silicon dioxide microspheres;
and 5, preparing the silica microspheres into a colloidal solution, and coating the colloidal solution on a glass sheet or a transparent film substrate to obtain the optically variable coating.
The invention is further improved in that:
preferably, in the step 1, the mixing volume ratio of the absolute ethyl alcohol, the deionized water and the ammonia water is (155-: (25-35): (3-10).
Preferably, in step 1, the mixing volume ratio of the absolute ethyl alcohol to the tetraethoxysilane is (155-): (4-6).
Preferably, in the step 1, the reaction temperature is 55-65 ℃ and the reaction time is 9-12 h.
Preferably, in the step 2, the mixing volume ratio of the absolute ethyl alcohol, the deionized water, the ammonia water and the reaction solution A is (155-: (25-35): (25-35): (1-10).
Preferably, in step 3, the volume of the tetraethoxysilane and the reaction solution C is equal.
Preferably, in the step 3, the reaction time is 4-5h, and the reaction temperature is 28-32 ℃.
Preferably, in step 4, the centrifugation speed is 4000-6000rpm, and the centrifugation time is 10 min.
Preferably, in the step 4, the drying temperature is 60-75 ℃, and the drying time is 8-16 h.
The optically variable coating prepared by the preparation method is formed by coating a colloidal solution, wherein the colloidal solution contains silica microspheres, and the particle size of the silica microspheres is 200-580 nm.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of an optically variable coating, which has the advantages of easily available raw materials, simple process, low cost, low energy consumption and easy realization, and takes tetraethoxysilane as a silicon source, absolute ethyl alcohol as a solvent and ammonia water as a catalyst to generate silicon dioxide particles with better monodispersity. Preparing a silica colloid solution with a certain mass fraction, and self-assembling the silica colloid solution on a transparent film substrate to generate the structural color of the silica photonic crystal. The whole preparation method is mild in reaction condition and easy to implement, the silicon dioxide microspheres with the particle size having the normal distribution characteristic are controllably prepared by adopting a precursor multi-step dropping method, the synthesis rate of silicon dioxide is controlled by bidirectional dropping in the reaction process, and finally the angle-dependent silicon dioxide photonic crystal is prepared. The structural color is changed in a circulating way in the whole visible light range, and the effect of iris dynamic transformation observed by naked eyes is realized.
The invention also discloses an optically variable coating which is prepared by coating silica microspheres on a glass plate or a transparent substrate, wherein the silica microspheres with different particle sizes are spherical, have good monodispersity and are angle-dependent silica photonic crystals, the photonic crystal coating moves along the direction vertical to the (111) crystal face, and the structural color of the coating changes cyclically in the whole visible light range along with the change of the incident light angle and the observation angle, so that the iridescence dynamic conversion effect observed by naked eyes is realized. The method has important guiding significance for the development of the colorful film for printing and packaging enterprises, and has potential market application prospect in the fields of optical devices, sensing, encryption, anti-counterfeiting and the like.
[ description of the drawings ]
FIG. 1 is a scanning electron micrograph of silica prepared according to example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of a silica photonic crystal prepared in example 1 of the present invention;
fig. 3 is a graph of the optically variable effect of the optically variable coating prepared in example 1 of the present invention under a point light source;
FIG. 4 is a reflection spectrum of a silica photonic crystal prepared in example 2 of the present invention;
FIG. 5 is a scanning electron microscope image of an optically variable coating prepared in example 3 of the present invention;
fig. 6 is a graph of the optically variable effect of the optically variable coating prepared in example 4 of the present invention under natural light;
FIG. 7 is a scanning electron micrograph of a silica photonic crystal prepared in example 6 of the present invention;
FIG. 8 is a laser particle size analysis chart of silica prepared in example 7 of the present invention.
[ detailed description ] embodiments
The invention is further described in detail by combining the drawings and the embodiment, and the invention discloses a preparation method of an optically variable coating, which specifically comprises the following steps:
(1) adding 165mL of anhydrous ethanol, 25-35mL of deionized water and 3-10mL of ammonia water into the three-mouth bottle; 4-6mL of tetraethyl orthosilicate (TEOS) is added dropwise, the reaction temperature is 55-65 ℃, the reaction time is 9-12h, and a reaction solution A is formed after hydrolysis and condensation reaction. In this step, the reaction solution A corresponds to a seed solution in which silica microspheres having a certain particle size are formed, so that these preliminarily formed silica microspheres can be used in the next step.
(2) Adding 165mL of anhydrous ethanol 155-165, 25-35mL of deionized water and 25-35mL of ammonia water into a three-necked bottle, stirring at low speed, and adding 1-10mL of the reaction solution A obtained in the step (1) to form a reaction solution B. In the step, the proportion of the silicon dioxide microspheres with different particle sizes in the finally formed reaction solution B can be adjusted by adjusting the adding amount of the reaction solution A, and SiO in the system is adjusted 2 And (4) colloidal microsphere dispersibility.
(3) Respectively dropwise adding equal amounts of TEOS solution and H into the solution B formed in the step (2) 2 O/Anhydrous ethanol/Ammonia Mixed solution C (H) 2 O, absolute ethyl alcohol, ammonia water 3: 10: 7) the TEOS solution and H 2 The dropping amount of the mixed solution C of O/absolute ethyl alcohol/ammonia water is 18-22mL, the dropping speed is 16-20mL/min, the synthesis speed of the silicon dioxide is controlled by a bidirectional dropping reagent, and the bidirectional dropping reagent is a TEOS solution and H 2 Reacting the mixed solution of O/absolute ethyl alcohol/ammonia water at the temperature of 28-32 ℃ for 4-5h to form a solution D.
(4) And (4) washing the solution C obtained in the step (3) with ethanol for 2-3 times, wherein the centrifugal rotation speed is 4000-6000rpm, the centrifugal time is 10min, and drying the centrifugal product at the temperature of 60-75 ℃ for 8-16h to obtain the silicon dioxide microspheres. The method can prepare the silica microspheres with multiple particle sizes at one time, and the particle size of the silica microspheres is between 200 and 580 nm.
(5) And (4) preparing a colloidal solution with the mass fraction of 0.1-1.5% by using the silicon dioxide microspheres obtained in the step (4). Self-assembly on a clean glass sheet or a transparent film substrate forms a photonic crystal structural color with an iridescent effect.
Example 1
(1) 160mL of absolute ethyl alcohol, 33mL of deionized water and 4mL of ammonia water are added into a three-mouth bottle; 4mL of Tetraethoxysilane (TEOS) is slowly added, the reaction temperature is 50 ℃, the reaction time is 12 hours, and the solution A is formed after the reaction is finished.
(2) Adding 160mL of absolute ethyl alcohol, 30mL of deionized water and 30mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding the solution A1mL obtained in the step (1), and continuously stirring to adjust the SiO in the system 2 And (4) dispersing the colloidal microspheres to form a solution B.
(3) Slowly injecting TEOS solution and H with equal amount into the solution B obtained in the step (2) 2 20mL of O/absolute ethyl alcohol/ammonia water mixed solution, the dropping speed of 20mL/min, the synthesis speed of silicon dioxide is controlled bidirectionally, and the reaction is carried out for 5h at 30 ℃ to form solution D.
(4) And (4) washing the solution C obtained in the step (3) for 3 times by using ethanol, wherein the centrifugal rotation speed is 5000rpm, the centrifugal time is 10min, and drying at 75 ℃ for 10h to obtain the silicon dioxide microspheres.
(5) And (4) preparing a colloidal solution with the mass fraction of 0.2% by using the silicon dioxide obtained in the step (4). Self-assembling on a clean glass sheet to form a photonic crystal structural color with an iridescence effect.
FIG. 1 is a scanning electron micrograph of the silica prepared in this example, from which it can be seen that the silica particles are in a regular spherical shape with a particle size distribution in the range of 200-500 nm.
FIG. 2 is a scanning electron micrograph of the silica photonic crystal prepared in this example.
Fig. 3 is a diagram of the optically variable effect of the optically variable coating prepared in example 1 under a point light source, and it can be seen that the color of the photonic crystal structure gradually changes from red to purple from left to right;
example 2
(1) 160mL of absolute ethyl alcohol, 33mL of deionized water and 4mL of ammonia water are added into a three-necked bottle; 4.2mL of tetraethyl orthosilicate (TEOS) was added slowly at 55 ℃ for 11h to form solution A after the reaction.
(2) Adding 155mL of absolute ethyl alcohol, 35mL of deionized water and 30mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding the solution A2mL obtained in the step (1), and continuously stirring to adjust SiO in the system 2 Dispersibility of the colloidal microspheres.
(3) Respectively and slowly injecting equal amount of TEOS solution and H into (2) 2 21mL of O/absolute ethyl alcohol/ammonia water mixed solution, the dropping speed is 17mL/min, the synthesis rate of the silicon dioxide is controlled bidirectionally, and the reaction is carried out for 4 hours at 30 ℃.
(4) And (4) washing the obtained product in the step (3) for 3 times by adopting ethanol, centrifuging at the rotating speed of 5000rpm for 10min, and drying at the temperature of 60 ℃ for 12h to obtain the silicon dioxide microspheres.
(5) And (4) preparing a colloidal solution with the mass fraction of 0.25% by using the silicon dioxide obtained in the step (4). Self-assembling to form photon crystal on the clean glass sheet and transparent film base material.
FIG. 4 is a reflection spectrum of the silica photonic crystal prepared in this example, from which it can be seen that the silica photonic crystal has reflection over the entire visible range.
Example 3
(1) 160mL of absolute ethyl alcohol, 33mL of deionized water and 4mL of ammonia water are added into a three-necked bottle; 4.4mL of tetraethyl orthosilicate (TEOS) was added slowly, the reaction temperature was 55 ℃ and the reaction time was 10h, forming a solution A after the reaction was over.
(2) Adding 155mL of absolute ethyl alcohol, 35mL of deionized water and 29mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 3mL of the reaction solution A obtained in the step (1), and continuously stirring to adjust SiO in the system 2 Dispersibility of the colloidal microspheres.
(3) Respectively and slowly injecting equal amount of TEOS solution and H into the chamber (2) 2 21mL of O/absolute ethyl alcohol/ammonia water mixed solution, the dropping speed is 16mL/min, the synthesis speed of the silicon dioxide is controlled bidirectionally, and the reaction is carried out for 5h at 30 ℃.
(4) And (4) washing the obtained product in the step (3) for 3 times by using ethanol, wherein the centrifugal rotation speed is 5000rpm, the centrifugal time is 10min, and drying at the temperature of 75 ℃ for 10h to obtain the silicon dioxide microspheres.
(5) And (4) preparing a colloidal solution with the mass fraction of 0.4% by using the silicon dioxide obtained in the step (4). Self-assembling on a clean glass sheet to form the photonic crystal.
FIG. 5 is a scanning electron micrograph of the silica photonic crystal prepared in this example. As can be seen from the figure, the silica particles with different particle sizes are spherical, and the particle size distribution range is 300-580 nm.
Example 4
(1) 150mL of absolute ethyl alcohol, 40mL of deionized water and 5mL of ammonia water are added into a three-neck bottle; 4.6mL of tetraethyl orthosilicate (TEOS) was slowly added, the reaction temperature was 58 ℃ and the reaction time was 11 hours, and a reaction solution A was formed after the reaction was completed.
(2) Adding 155mL of absolute ethyl alcohol, 35mL of deionized water and 28mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 1mL of the reaction solution A obtained in the step (1), continuously stirring, and adjusting SiO in a system 2 Dispersibility of the colloidal microspheres.
(3) Respectively and slowly injecting equal amount of TEOS solution and H into the chamber (2) 2 18mL of O/absolute ethyl alcohol/ammonia water mixed solution, wherein the dripping speed is 18mL/min, the synthesis speed of silicon dioxide is bidirectionally controlled, and the reaction is carried out for 5h at room temperature.
(4) And (4) washing the obtained product in the step (3) for 3 times by using ethanol, wherein the centrifugal rotation speed is 5000rpm, the centrifugal time is 10min, and drying at the temperature of 75 ℃ for 10h to obtain the silicon dioxide microspheres.
(5) And (4) preparing a colloidal solution with the mass fraction of 0.6% by using the silicon dioxide obtained in the step (4), and self-assembling on a clean glass sheet to form the photonic crystal.
Fig. 6 is a graph showing the optical variation effect of the optical variation coating prepared in this embodiment moving along the direction perpendicular to the (111) crystal plane under natural light. It can be seen that from left to right, the color of the photonic crystal structure changes from red to purple to realize the rainbow color gradual change effect.
Example 5
(1) 150mL of absolute ethyl alcohol, 40mL of deionized water and 5mL of ammonia water are added into a three-necked bottle; 4.6mL of Tetraethoxysilane (TEOS) is slowly added, the reaction temperature is 60 ℃, the reaction time is 10 hours, and a reaction solution A is formed after the reaction is finished.
(2) Adding 150mL of absolute ethyl alcohol, 30mL of deionized water and 28mL of ammonia water into a three-necked bottle, stirring at a low rotating speed, adding 2mL of the reaction solution A obtained in the step (1), continuously stirring, and adjusting SiO in a system 2 Dispersibility of the colloidal microspheres.
(3) Respectively and slowly injecting equal amount of TEOS solution and H into the chamber (2) 2 18mL of O/absolute ethyl alcohol/ammonia water mixed solution, wherein the dripping speed is 18mL/min, the synthesis speed of silicon dioxide is bidirectionally controlled, and the reaction is carried out for 4 hours at room temperature.
(4) And (4) washing the obtained product in the step (3) for 2 times by using ethanol, wherein the centrifugal rotation speed is 5000rpm, the centrifugal time is 10min, and drying at 60 ℃ for 12h to obtain the silicon dioxide microspheres.
(5) And (4) preparing a colloidal solution with the mass fraction of 0.3% by using the silicon dioxide obtained in the step (4). Self-assembling on a clean glass sheet to form the photonic crystal.
Example 6
(1) Adding 155mL of absolute ethyl alcohol, 35mL of deionized water and 5mL of ammonia water into a three-necked bottle, wherein the total volume is 200 mL; 4.7mL of Tetraethoxysilane (TEOS) is slowly added, the reaction temperature is 58 ℃, the reaction time is 11 hours, and a reaction solution A is formed after the reaction is finished.
(2) Adding 155mL of absolute ethyl alcohol, 30mL of deionized water and 28mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 2mL of the reaction solution A obtained in the step (1), continuously stirring, and adjusting SiO in a system 2 And (4) colloidal microsphere dispersibility.
(3) Respectively and slowly injecting equal amount of TEOS solution and H into the chamber (2) 2 19mL of O/absolute ethyl alcohol/ammonia water mixed solution, the dropping speed is 19mL/min, the synthesis rate of the silicon dioxide is controlled bidirectionally, and the reaction is carried out for 5 hours at room temperature.
(4) And (4) washing the obtained product in the step (3) for 2 times by adopting ethanol, wherein the centrifugal rotating speed is 5000rpm, the centrifugal time is 10min, and drying at the temperature of 60 ℃ for 12h to obtain the silicon dioxide microspheres.
(5) And (4) preparing a colloidal solution with the mass fraction of 0.8% by using the silicon dioxide obtained in the step (4), and carrying out self-assembly on a clean glass sheet to form the photonic crystal.
FIG. 7 is a scanning electron micrograph of the silica prepared in this example. As can be seen, the prepared silica has a particle size distribution of 400-680 nm.
Example 7
(1) Adding 155mL of absolute ethyl alcohol, 40mL of deionized water and 5mL of ammonia water into a three-necked bottle; 4.8mL of Tetraethoxysilane (TEOS) is slowly added, the reaction temperature is 55 ℃, the reaction time is 9 hours, and a reaction solution A is formed after the reaction is finished.
(2) Adding 160mL of absolute ethyl alcohol, 30mL of deionized water and 28mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 1mL of the reaction solution A obtained in the step (1), continuously stirring, and adjusting SiO in a system 2 Dispersibility of the colloidal microspheres.
(3) Into (2)The same amount of TEOS solution and H are slowly injected respectively 2 18mL of O/absolute ethyl alcohol/ammonia water mixed solution, the dripping speed of 18mL/min, the synthesis speed of silicon dioxide, and the reaction time of 5h at room temperature.
(4) And (4) washing the obtained product in the step (3) for 3 times by using ethanol, wherein the centrifugal rotation speed is 5000rpm, the centrifugal time is 10min, and drying at the temperature of 75 ℃ for 10h to obtain the silicon dioxide microspheres.
(5) And (4) preparing a colloidal solution with the mass fraction of 0.4% by using the silicon dioxide obtained in the step (4). Self-assembling on a clean glass sheet to form the photonic crystal.
FIG. 8 is a graph showing the particle size analysis of the silica prepared in this example. As can be seen from the figure, the particle size distribution of the prepared silica is in the range of 200-600nm and is in normal distribution.
Example 8
(1) 160mL of absolute ethyl alcohol, 30mL of deionized water and 5.2mL of ammonia water are added into a three-mouth bottle; 4.8mL of tetraethyl orthosilicate (TEOS) is slowly added, the reaction temperature is 60 ℃, the reaction time is 9 hours, and a reaction solution A is formed after the reaction is finished.
(2) Adding 160mL of absolute ethyl alcohol, 28mL of deionized water and 28mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 3mL of the reaction solution A obtained in the step (1), continuously stirring, and adjusting SiO in a system 2 Dispersibility of the colloidal microspheres.
(3) Respectively and slowly injecting equal amount of TEOS solution and H into the chamber (2) 2 18mL of O/absolute ethyl alcohol/ammonia water mixed solution, the dropping speed is 18mL/min, the synthesis rate of the silicon dioxide is controlled bidirectionally, and the reaction is carried out for 5 hours at room temperature.
(4) And (4) washing the obtained product in the step (3) for 3 times by using ethanol, wherein the centrifugal rotation speed is 5000rpm, the centrifugal time is 10min, and drying at 70 ℃ for 11h to obtain the silicon dioxide microspheres.
(5) And (4) preparing a colloidal solution with the mass fraction of 0.4% by using the silicon dioxide obtained in the step (4). Self-assembling on a clean glass sheet to form the photonic crystal.
Example 9
(1) Adding 155mL of absolute ethyl alcohol, 35mL of deionized water and 5.2mL of ammonia water into a three-necked bottle; 4.8mL of tetraethyl orthosilicate (TEOS) is slowly added, the reaction temperature is 55 ℃, the reaction time is 9 hours, and a reaction solution A is formed after the reaction is finished.
(2) Adding 155mL of absolute ethyl alcohol, 35mL of deionized water and 28mL of ammonia water into a three-neck flask, stirring at a low rotating speed, adding 3mL of the reaction solution A obtained in the step (1), continuously stirring, and adjusting SiO in a system 2 And (4) colloidal microsphere dispersibility.
(3) Respectively and slowly injecting equal amount of TEOS solution and H into the chamber (2) 2 21mL of O/absolute ethyl alcohol/ammonia water mixed solution, the dropping speed is 20mL/min, the synthesis rate of the silicon dioxide is controlled bidirectionally, and the reaction time is 4-5h at room temperature.
(4) And (4) washing the obtained product in the step (3) for 3 times by using ethanol, wherein the centrifugal rotation speed is 5000rpm, the centrifugal time is 10min, and drying at the temperature of 75 ℃ for 10h to obtain the silicon dioxide microspheres.
(5) And (5) preparing a colloidal solution with the mass fraction of 0.8% by using the silicon dioxide obtained in the step (4). Self-assembling on a clean glass sheet to form the photonic crystal.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. The preparation method of the optically variable coating is characterized by comprising the following steps:
step 1, mixing absolute ethyl alcohol, deionized water and ammonia water, adding tetraethoxysilane, and reacting to generate a reaction solution A;
the mixing volume ratio of the absolute ethyl alcohol, the deionized water and the ammonia water is (155-): (25-35): (3-10);
the mixing volume ratio of the anhydrous ethanol to the ethyl orthosilicate is (155-: (4-6);
step 2, mixing absolute ethyl alcohol, deionized water and ammonia water, and then dropwise adding the reaction solution A to form a reaction solution B; the mixing volume ratio of the absolute ethyl alcohol, the deionized water, the ammonia water and the reaction solution A is (155-: (25-35): (25-35): (1-10);
step 3, adding absolute ethyl alcohol and ammonia water into water to form a reaction solution C; dropwise adding ethyl orthosilicate and the reaction solution C into the reaction solution B, and reacting to generate a solution D; the volume of the ethyl orthosilicate is equal to that of the reaction solution C;
step 4, washing the solution D with ethanol, centrifuging, and drying the centrifuged product to obtain silicon dioxide microspheres;
and 5, preparing the silica microspheres into a colloidal solution, and coating the colloidal solution on a glass sheet or a transparent film substrate to obtain the optically variable coating.
2. The method for preparing an optically variable coating according to claim 1, wherein the reaction temperature in step 1 is 55-65 ℃ and the reaction time is 9-12 h.
3. A method for preparing an optically variable coating according to claim 1, wherein in step 3, the reaction time is 4-5h and the reaction temperature is 28-32 ℃.
4. The method as claimed in claim 1, wherein the centrifugation speed is 4000-6000rpm and the centrifugation time is 10min in step 4.
5. The method for preparing an optically variable coating according to claim 1, wherein in step 4, the drying temperature is 60-75 ℃ and the drying time is 8-16 h.
6. An optically variable coating prepared by the preparation method of any one of claims 1 to 5, wherein the optically variable coating is formed by coating a colloidal solution, silica microspheres are contained in the colloidal solution, and the particle size of the silica microspheres is 200-580 nm.
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